Preparation method of a multifunctional highly visible fabric

By modifying polyester-cotton blended fabrics and using specific additives to prepare fluorine-free waterproof and anti-fouling finishing agents, combining persimmon paint and pigment to form a slurry, and after ultraviolet curing, the existing high-visibility fabric lacks waterproof, anti-fouling and moisture permeability functions in outdoor applications, achieving good waterproof, anti-fouling and moisture permeability functions of the fabric and stronger applicability.

CN119843483BActive Publication Date: 2025-06-20FUKE NEW MATERIALS (SHANGHAI) CO LTD
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Patent Information

Application Number
CN202510344462.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-21
Publication Date
2025-06-20
Estimated Expiration
2045-03-21

AI Technical Summary

Technical Problem

The existing high-visibility fabrics lack waterproof, stain-proof and moisture-permeable functions in outdoor applications, resulting in insufficient comfort for the wearer.

Method used

By modifying the polyester-cotton blended fabric, and using guar gum, nanosilica and other additives to prepare a fluorine-free waterproof and anti-fouling finishing agent, combined with persimmon paint and pigment to form a slurry, and after ultraviolet curing treatment, a high-visual fabric with fluorescence properties, wash-resistant and durable properties are prepared.

Benefits of technology

It realizes the good waterproof, stain-proof and moisture-permeable function of the fabric, while maintaining hygroscopicity and wash resistance, stronger applicability, and relatively low temperature, avoiding the negative impact on the fluorescent performance and feel of the fabric.

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Abstract

The present application provides a preparation method of a multifunctional highly visible fabric, belonging to the technical field of functional textiles. A modifier is prepared by adding sodium hydroxide, cellulose complex enzyme, penetrant and water. After the polyester-cotton blended fabric is impregnated in the modifier and subjected to impregnation treatment, it is washed with water until neutral and then dried to obtain a modified fabric. Using guar gum and nano-silica as monomers, acrylic acid, butyl acrylate, sodium dodecyl sulfate and water are added and stirred to obtain a monomer emulsion. The monomer emulsion is reacted with an initiator to obtain a polyacrylate emulsion, and sodium dodecylbenzenesulfonate, emulsifier and acryloxypropyl caged polyhedral oligomeric silsesquioxane are added and reacted to obtain a finishing agent. A slurry obtained by mixing pigments, persimmon lacquer and the finishing agent is coated on the modified fabric and subjected to ultraviolet curing treatment. This process uses a relatively low temperature to achieve good waterproof performance, avoids the influence of high-temperature baking on the fluorescence performance and hand feeling of the fabric, and saves energy.
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Description

Technical Field

[0001] The present application relates to a preparation method of a multifunctional highly visible fabric, belonging to the technical field of functional textiles. Background Art

[0002] In recent years, with the development of science and technology and the improvement of people's living standards, the market demand for functional and intelligent textile products has been increasing continuously, and the market demand for products such as comfort, health, and safety protection has been growing day by day. Among them, functional protective highly visible clothing is made of a substrate material with a prominent color and a material with luminescence or reflectivity. In situations with extremely poor visibility such as at night, heavy rain, heavy snow, sandstorms, and fog, it can not only significantly distinguish the wearer from the surrounding environment, play a warning role for others, and avoid accidents, but also be widely used in traffic police, road surveyors, sanitation workers, road administration and greening workers, as well as night running clothes, festival and stage costumes, etc. At present, there are many studies on highly visible warning fabrics, but for outdoor application environments, waterproof, anti-fouling, and moisture permeability are very crucial for improving the comfort of the wearer. However, there are few research reports on functional fabrics with waterproof, anti-fouling, and moisture permeability functions, resulting in significant defects in the application of visible fabrics. Summary of the Invention

[0003] In view of this, the present application provides a preparation method of a multifunctional highly visible fabric, which not only meets the required fluorescent color and wet treatment fastness, but also has good waterproof, anti-fouling, and moisture permeability functions, and has stronger applicability.

[0004] Specifically, the present application is realized through the following scheme:

[0005] A preparation method of a multifunctional highly visible fabric, taking a polyester-cotton blended fabric as the treatment object, and performing the following treatments:

[0006] Step 1, preparing a modifier by adding sodium hydroxide, cellulose complex enzyme, penetrant and water, impregnating the polyester-cotton blended fabric in the modifier, washing it with water until neutral, and drying it to obtain a modified fabric;

[0007] Step 2, using 0.5-10% guar gum and 0.2-1% nano-silica as monomers, adding 1-5% acrylic acid, 1-5% butyl acrylate, 1-5% sodium dodecyl sulfate, and water, and stirring to obtain a monomer emulsion; adding 0.5-1% initiator to the monomer emulsion for reaction to obtain a polyacrylate emulsion, adjusting the pH of the emulsion to 6-7 after the reaction ends, and adding 1-10% sodium dodecylbenzenesulfonate, 2-20% acryloyloxypropylcaged polyhedral oligomeric silsesquioxane and the remaining emulsifier, stirring and reacting at room temperature, filtering, and centrifuging to remove impurities to obtain a fluorine-free waterproof and anti-fouling finishing agent;

[0008] Step 3: Mix the pigment, persimmon lacquer, the fluorine-free waterproof and antifouling finishing agent obtained in Step 2, and deionized water to obtain a slurry. Apply the obtained slurry onto the modified fabric obtained in Step 1, and perform ultraviolet curing treatment to obtain the finished product.

[0009] In the above solution, the polyester-cotton blended fabric is first subjected to modified pretreatment, and then the slurry formed by the finishing agent, pigment, and persimmon lacquer is applied. The coating is completed by the single-sided printing method, and then baked to obtain the finished product. The obtained product is a highly visible fabric with fluorescence performance, wash resistance, and durability. This fabric not only meets the required fluorescent color and wet treatment fastness but also has good waterproof, antifouling, and moisture-permeable functions.

[0010] Further, as a preference:

[0011] In Step 1,

[0012] The mass percentages of the components in the modifier are as follows:

[0013] Sodium hydroxide concentration: 1 - 10 g / L,

[0014] Cellulose complex enzyme concentration: 1 - 5 g / L,

[0015] Penetrant concentration: 0.5 - 2 g / L,

[0016] Bath ratio 1:50.

[0017] The temperature of the impregnation treatment is 40 - 60 °C, and the duration is 1 - 3 h.

[0018] The drying temperature is 60 - 80 °C, and the drying duration is 20 - 30 min.

[0019] In Step 2,

[0020] The mass ratio of guar gum to nano-silica is 4:1 - 1:4.

[0021] The reaction conditions of the polyacrylate emulsion are: under nitrogen protection, react at 70 - 90 °C for 3 - 5 h.

[0022] In Step 3,

[0023] In the slurry, the mass percentages of the components are:

[0024] Pigment: 1 - 5%,

[0025] Persimmon lacquer: 1 - 12%,

[0026] Fluorine-free waterproof and antifouling finishing agent: 10 - 30%,

[0027] The balance is deionized water.

[0028] The pigment is one of fluorescent yellow or fluorescent orange.

[0029] The pre-baking temperature after coating is 60-80°C, and the duration is 10-30 min.

[0030] UV curing treatment: intensity 40-45.0 W / m 2 , temperature 20-45°C, and duration 1-5 h.

[0031] The fabric obtained by the above scheme not only has good waterproof and stain-proof properties, but also maintains the original good moisture absorption of the polyester-cotton blended fabric, and has excellent washability; the fabric is prepared by low-temperature UV curing treatment after coating finishing. This process uses a relatively low temperature to achieve good waterproof performance, avoiding the influence of high-temperature baking on the fluorescence performance and hand feeling of the fabric. While saving energy, it has little influence on the fluorescence performance, hand feeling and color change of the fabric. Description of the Drawings

[0032] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings required for use in the embodiments or the description of the prior art. Obviously, the following drawings are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0033] Figure 1 Scanning electron microscope images of the fabric before and after finishing;

[0034] Figure 2 Infrared spectra of the fabric before and after finishing. Specific Embodiments

[0035] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application more clearly understood, the following will further elaborate on the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the technical solutions of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present application.

[0036] Testing method:

[0037] Fluorescence performance evaluation method: Refer to the method in GB 20653-2006 "High-visibility warning clothing for occupational use" for evaluation, and measure using a Datacolor 600 computer color measurement and matching instrument with a D65 light source and a 2° field of view angle. The fluorescent yellow color should be within the color range specified by the national standard, and its minimum luminance coefficient β should exceed 0.70.

[0038] The waterproofness test was carried out according to "Testing and Evaluation of Waterproof Performance of Textiles - Spray Test" (GB / T 4745-2012) to test the waterproof performance of textiles. The higher the grade, the better the performance.

[0039] The stain resistance performance was tested according to "Testing and Evaluation of Antisoiling Performance of Textiles - Part 1: Resistance to Soiling" (GB / T 30159.1-2013). In addition to the high-salt thin soy sauce specified in the standard, corn oil was selected for the same test. The higher the grade, the better the performance.

[0040] Water absorption rate: The test specimen was placed in a container filled with tertiary water. After the specimen absorbed water and sank naturally, it was taken out after being completely wetted for 5 min, and was hung vertically in a natural and flat state. The water on the specimen dripped naturally. When the specimen no longer dripped water, the weight of the specimen was immediately weighed accurately to 0.001 g. Repeat three times and take the average value. The formula for calculating the water absorption rate is:

[0041] A (%) = (m - m0) / m0 × 100.

[0042] Where A is the water absorption rate, m0 is the original mass of the test specimen, and m is the mass of the specimen after being completely wetted.

[0043] Droplet diffusion: After the test specimen was equilibrated in the standard atmosphere for 24 h, 0.2 mL of water was dropped vertically at 90° on the test specimen, and the time required for the water droplet to contact the surface of the test specimen until it was completely diffused was recorded accurately to 0.1 s. Repeat 5 times and calculate the average value.

[0044] Textile color fastness: According to "Textiles - Tests for Color Fastness - Color Fastness to Rubbing" (GB / T 3920-2024), the color transfer of textiles in dry and wet states was tested. According to the standard of "Textiles - Tests for Color Fastness - Color Fastness to Water" (GB / T 5713-2013), the color retention ability of textiles under washing conditions was tested.

[0045] The hand feeling test was carried out with reference to the AATCC EP5-2011 Fabric Hand Evaluation Procedure. The treated test specimen was compared with the original specimen, and the feeling level was described according to the change in hand feeling. Level 1 means no different feeling; Level 2 means a slight different feeling; Level 3 means a moderate different feeling; Level 4 means an obvious difference is felt.

[0046] Example 1

[0047] The preparation method of the multifunctional highly visible fabric in this example is as follows:

[0048] Step 1, modification treatment:

[0049] A modifier was prepared by mixing 5 g / L of sodium hydroxide, 4 g / L of cellulose complex enzyme (model Celluclast), 1 g / L of penetrant JFC and deionized water. A 65 / 35 polyester-cotton blended fabric was impregnated in the modifier at 50 °C for 1 h with a bath ratio of 1:50. After impregnation, the fabric was thoroughly washed three times with deionized water until neutral and then dried at 80 °C for 30 min to obtain the modified fabric.

[0050] Step two, prepare the finishing agent:

[0051] 1) Using 3.5 g of guar gum, 6.5 g of sodium dodecyl sulfate, and 0.8 g of nano-silica as monomers, 3.2 g of butyl acrylate, 7.4 g of acrylic acid and 70 mL of deionized water were added and stirred well to dissolve. Then, it was stirred at 900 revolutions per minute for 30 min to obtain a pre-emulsified monomer emulsion.

[0052] 2) The monomer emulsion was added to a reaction kettle, and 1.7 g of potassium persulfate was added as an initiator. Under nitrogen protection, a polymerization reaction was carried out at 70 °C for 4 h to obtain a polyacrylate emulsion.

[0053] 3) After the polymerization reaction was completed, the pH value of the emulsion was adjusted to 7. 1.5 g of sodium dodecylbenzenesulfonate, 1.5 g of Tween 80 and 15 g of acryloxypropylcaged polyhedral oligomeric silsesquioxane were added, and it was stirred at room temperature for 3 h. Finally, through filtration and centrifugation, the solid impurities in the emulsion were removed to obtain a fluorine-free waterproof and antifouling finishing agent.

[0054] Step three, one-sided scraping and finishing:

[0055] A slurry was prepared by uniformly stirring and mixing 2% fluorescent yellow, 8% persimmon lacquer, 0.8% nano-silica, 30% fluorine-free waterproof and antifouling finishing agent, and 59.2% deionized water by mass percentage. Using an 80-mesh screen frame, the slurry was coated once on the modified fabric obtained in step one with a rubber squeegee. The treated fabric was placed in an 80 °C oven and dried for 20 min, and then subjected to ultraviolet curing treatment at 40 °C and 45.0 W / m 2 for 5 h to obtain a waterproof, antifouling, moisture-absorbing and highly visible fabric.

[0056] Figure 1 The following are the electron scanning microscope images of the fabric before and after finishing: The surface of the untreated fabric is smooth and no other substances are adhered. The arrangement of the yarns is relatively loose; after finishing, a covering layer can be seen on the yarns of the fabric, and there are granular substances. The surface of the yarns is rougher than that of the untreated fabric. It shows that the finishing agent is wrapped on the surface of the yarns, and the nano-silica aggregates on the surface of the yarns to form a micro-nano rough structure, increasing the water contact angle, thereby improving the waterproof and antifouling ability of the fabric.

[0057] Figure 2Infrared spectra of the front and back fabrics before finishing: The original unprocessed fabric shows a broad and strong absorption peak at 3336 cm -1 with a medium-intensity absorption peak at 1650 cm -1 appearing, which are characteristic of the hydroxyl groups in cellulose. For the finished fabric, the absorption peaks at these two positions are significantly weakened or shifted. A new absorption peak appears at 1720 cm -1 for the finished fabric, which is a typical characteristic of the carbonyl group of esters; a new absorption peak appears at 2322 cm -1 for the stretching vibration of the silicon-hydrogen bond (Si-H); a new absorption peak appears at 1271 cm -1 for the stretching absorption peak of the silicon-oxygen bond (Si-O). This indicates that the hydroxyl groups on the finished fabric are blocked or reacted by the finishing agent, resulting in a decrease in their quantity. At the same time, a new siloxane structure appears, and the finishing agent reacts with the fabric and exists on the fabric.

[0058] The obtained fabric was tested for performance. The water absorption rate was 198%, the water droplet diffusion time was 10.2 s, the breaking strength was 165 N, the brightness coefficient β was 0.73, and both the waterproofness and stain resistance reached grade 5.

[0059] Comparative Example 1

[0060] This comparative example was set up the same as Example 1, except that: before single-sided scraping finishing, the polyester-cotton blended fabric was not subjected to modification treatment.

[0061] Table 1: Influence of modification on the finishing effect

[0062] .

[0063] The fabric was modified using sodium hydroxide and cellulase to remove residual impurities and oil stains on the fabric, improve the hydrophilic properties of the fabric, and enhance its binding ability with the finishing agent. Therefore, compared with Comparative Example 1, under the same conditions, Example 1 showed improvements in water absorption rate, water droplet diffusion time, brightness coefficient, and waterproofness, while the breaking strength decreased slightly.

[0064] Comparative Example 2

[0065] This comparative example was set up the same as Example 1, except that: in Step 3, persimmon varnish was not added, and only a commercially available fluorine-free finishing agent (RUCO-DRY ECO PLUS) was added.

[0066] Table 2: Influence of the finishing agent

[0067] .

[0068] In Comparative Example 2, the self-made waterproofing finishing agent and persimmon lacquer were not added. Compared with Example 1, its brightness coefficient was lower, not meeting the requirements of the high-visibility national standard. The waterproofness, soil resistance, color fastness to washing, and color fastness to rubbing were all lower than those of Example 1. Adding persimmon lacquer is beneficial to the uniform dispersion of pigments in the emulsion and has the function of a cross-linking agent. It synergistically acts with the self-made finishing agent on the fabric to improve the fluorescence performance and waterproofness of the fabric, and the fabric has good color fastness.

[0069] Example 2

[0070] This example is the same as the setting of Example 1, except that the concentrations of sodium hydroxide and cellulase are different, as shown in Table 3 specifically.

[0071] Table 3: Influence of different mass ratios of sodium hydroxide to cellulase on fabric properties

[0072] 。

[0073] It can be seen from Table 3 that with the increase in the concentration of sodium hydroxide, the water absorption rate of the modified fabric continuously increases; with the increase in the proportion of cellulase, the water droplet diffusion property continuously increases. The treatment with sodium hydroxide has an etching effect on the polyester component and can cause the swelling of the cotton fiber component at the same time, jointly improving the hydrophilicity of the fabric. Its synergy with cellulase not only removes the hydrophobic impurities on the fabric surface but also reduces the crystallinity of the fibers in the fabric. The concentrations of sodium hydroxide and cellulase should be controlled within the range of 5 g / L and 4 g / L. At this time, the water absorption rate and water droplet diffusion property perform well, and the breaking strength meets the usage requirements.

[0074] Example 3

[0075] This example is the same as the setting of Example 1, except that the modification temperature is replaced by 40°C, 45°C, 55°C, and 60°C respectively, as shown in Table 4 specifically.

[0076] Table 4: Influence of modification temperature on fabric properties

[0077] 。

[0078] It can be seen from Table 4 that the modification treatment temperature should not be too high. When the treatment temperature exceeds 50°C, it will cause a decrease in the fabric strength and affect its wearing performance. The modification temperature is preferably controlled at 50 - 55°C.

[0079] Example 4

[0080] This example is the same as the setting of Example 1, except that the mass percentage of persimmon lacquer is replaced by 1%, 2%, 5%, and 10% respectively, as shown in Table 5 specifically.

[0081] Table 5: Influence of mass percentage of persimmon lacquer on fabric properties

[0082] 。

[0083] As can be seen from Table 5, as the concentration of persimmon lacquer increases, the brightness coefficient of the functional fabric continuously improves. When the mass percentage of persimmon lacquer is 8%, it can meet the requirements of high-visibility fabrics, and it has good waterproof and stain-resistant properties, and the hand feeling remains unchanged. However, when the mass percentage of persimmon lacquer exceeds 8%, the brightness coefficient decreases instead, the fluorescence performance of the fabric becomes poor, and the hand feeling of the fabric becomes poor. Persimmon lacquer is a natural polymer, which can form a film under certain conditions and has good waterproof performance. Persimmon lacquer contains polar groups such as hydroxyl groups. Appropriate addition can improve the dispersion uniformity of fluorescent pigments and improve the fluorescence performance of the fabric. However, when the concentration is too high, the polymerization of persimmon lacquer into a high polymer will instead affect the fluorescence performance of the fabric, and the fabric hand feeling becomes hard. Therefore, the addition amount of persimmon lacquer is preferably controlled at 8%.

[0084] Example 5

[0085] This example is the same as the setting of Example 1, except that the added mass percentage of the fluorine-free waterproof and stain-resistant finishing agent is replaced by 5%, 10%, 20%, and 50% respectively, as shown in Table 6 specifically.

[0086] Table 6: Influence of modification temperature on fabric properties

[0087] 。

[0088] As can be seen from Table 6, as the dosage of the fluorine-free waterproof and stain-resistant finishing agent increases, the waterproof and stain-resistant properties of the fabric are significantly improved, and the fluorescence performance (brightness coefficient β) changes little. Guar gum is a derivative of a natural polymer, with film-forming and adhesion properties similar to those of macromolecular polymers. The hydroxyl groups and hydrogen bonds in its structure can have a good binding force with the fabric, and it has good water and stain repellent properties. Adding nano-titanium dioxide can form raised microstructures on the fabric surface, further improving the waterproof performance. When the dosage of the fluorine-free waterproof and stain-resistant finishing agent is greater than 30%, the fluorescence performance of the fabric decreases. This may be because the surface coating of the fabric is thicker, reducing its flexibility and fluorescence performance. Therefore, in the sizing agent, the added amount of the fluorine-free waterproof and stain-resistant finishing agent is preferably controlled at 10 - 30%, and it is better at 20 - 30%.

[0089] Example 6

[0090] This example is the same as the setting of Example 1, except that the ultraviolet curing temperature is replaced by 20°C, 30°C, 35°C, and 45°C respectively, as shown in Table 7 specifically, and compared with the conventional high-temperature baking process (150°C, 1 min).

[0091] Table 7: Influence of ultraviolet curing temperature on fabric properties

[0092] 。

[0093] It can be seen from Table 7 that as the curing temperature increases, the waterproofness and stain resistance of the fabric gradually improve, and the fluorescence performance changes little. Compared with the traditional baking process, the ultraviolet curing treatment can achieve better waterproof performance at a relatively low temperature, avoiding the influence of high-temperature baking on the fluorescence performance and hand feeling of the fabric and saving energy.

[0094] The above-described embodiments only represent several feasible implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the patent of the present invention. The embodiments are not intended to limit the scope of protection in the claims of the present invention. For those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made. Any equivalent implementation or change made without departing from the present invention should be included in the technology of the present invention.

Claims

1. A method for preparing a multifunctional high-visibility fabric, characterized in that: Take polyester-cotton blended fabric as the treatment object and carry out the following treatment: Step 1: prepare a modifier by adding sodium hydroxide, cellulose complex enzyme, and penetrant into water, immerse the polyester-cotton blended fabric in the modifier, wash it with water until it is neutral, and dry it. The mass percentages of the components in the modifier are as follows: Sodium hydroxide concentration: 1-10 g / L, Cellulose complex enzyme concentration: 1-5 g / L, Osmotic agent concentration: 0.5-2 g / L, Bath ratio 1:50, The immersion temperature is 40-60°C and the duration is 1-3 hours; Step 2: adding 1-5% acrylic acid, 1-5% butyl acrylate, 1-5% sodium dodecyl sulfate and water to 0.5-10% guar gum and 0.2-1% nano-silica, and stirring to obtain a monomer emulsion; adding 0.5-1% initiator to the monomer emulsion to react to obtain a polyacrylate emulsion, adjusting the pH of the emulsion to 6-7 after the reaction is completed, and adding 1-10% sodium dodecylbenzene sulfonate, 2-20% acryloxypropyl caged polysilsesquioxane and an emulsifier, stirring to react at room temperature, filtering, and centrifuging to remove impurities to obtain a fluorine-free waterproof and antifouling finishing agent; Step three, mixing the pigment, persimmon paint, the fluorine-free waterproof and antifouling finishing agent obtained in step two and deionized water to obtain a slurry, applying the obtained slurry on the fabric obtained by drying in step one, and performing ultraviolet curing to obtain a finished product.

2. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: The concentration ratio of sodium hydroxide to cellulose complex enzyme is 2 to 1:

1.

3. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: In step 1, the drying temperature is 60-80° C. and the drying time is 20-30 minutes.

4. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: In step 2, under nitrogen protection, the reaction is carried out at 70-90° C. for 3-5 hours to obtain a polyacrylate emulsion.

5. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: In the slurry, the mass percentage of each component is: Pigment: 1-5%, Persimmon paint: 1-12%, Fluorine-free water-repellent and antifouling finishing agent: 10-30%, The balance was deionized water.

6. A method for preparing a multifunctional high-visibility fabric according to claim 1 or 5, characterized in that: The pigment is fluorescent yellow or fluorescent orange.

7. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: The ultraviolet curing intensity is 40 to 45.0 W / m 2 , temperature 20 ~ 45 ℃, duration 1 ~ 5h.

8. The method for preparing a multifunctional high-visibility fabric according to claim 1, characterized in that: After coating, pre-baking is performed at a temperature of 60 to 80°C, and ultraviolet curing is performed after pre-baking for 10 to 30 minutes.

Citation Information

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